US20030198837A1 - Non-polar a-plane gallium nitride thin films grown by metalorganic chemical vapor deposition - Google Patents

Non-polar a-plane gallium nitride thin films grown by metalorganic chemical vapor deposition Download PDF

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US20030198837A1
US20030198837A1 US10/413,691 US41369103A US2003198837A1 US 20030198837 A1 US20030198837 A1 US 20030198837A1 US 41369103 A US41369103 A US 41369103A US 2003198837 A1 US2003198837 A1 US 2003198837A1
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substrate
plane
gallium nitride
overscore
thin film
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Michael Craven
James Speck
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University of California
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Assigned to REGENTS OF THE UNIVERSITY OF CALIFORNIA, THE reassignment REGENTS OF THE UNIVERSITY OF CALIFORNIA, THE ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: CRAVEN, MICHAEL D., SPECK, JAMES S.
Publication of US20030198837A1 publication Critical patent/US20030198837A1/en
Priority to AU2003293497A priority patent/AU2003293497A1/en
Priority to EP03790447A priority patent/EP1697965A4/fr
Priority to US10/582,390 priority patent/US20070128844A1/en
Priority to PCT/US2003/039355 priority patent/WO2005064643A1/fr
Priority to JP2005512863A priority patent/JP5096677B2/ja
Priority to CN2003801109995A priority patent/CN1894771B/zh
Priority to US11/140,893 priority patent/US7208393B2/en
Priority to US13/151,491 priority patent/US9039834B2/en
Priority to US14/921,734 priority patent/US9893236B2/en
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Definitions

  • the invention is related to semiconductor materials, methods, and devices, and more particularly, to non-polar a-plane gallium nitride (GaN) thin films grown by metalorganic chemical vapor deposition (MOCVD).
  • GaN gallium nitride
  • MOCVD metalorganic chemical vapor deposition
  • Nitride-based optoelectronic and electronic devices are subject to polarization-induced effects because they employ nitride films grown in the polar c-direction [0001], the axis along which the spontaneous and piezoelectric polarization of nitride films are aligned. Since the total polarization of a nitride film depends on the composition and strain state, discontinuities exist at interfaces between adjacent device layers and are associated with fixed sheet charges that give rise to internal electric fields.
  • Polarization-induced electric fields although advantageous for two-dimensional electron gas (2DEG) formation in nitride-based transistor structures, spatially separate electrons and hole wave functions in quantum well (QW) structures, thereby reducing carrier recombination efficiencies in QW based devices, such as laser diodes and light emitting diodes.
  • QW quantum well
  • a potential means of eliminating the effects of these polarization-induced fields is through the growth of structures in directions perpendicular to the GaN c-axis (non-polar) direction.
  • m-plane AlGaN/GaN quantum wells have recently been grown on lithium aluminate substrates via plasma-assisted molecular beam epitaxy (MBE) without the presence of polarization-induced electric fields along the growth direction. See Reference 8.
  • a-plane nitride semiconductors also provides a means of eliminating polarization-induced electric field effects in wurtzite nitride quantum structures.
  • a-plane GaN growth had been achieved on r-plane sapphire via MOCVD and molecular beam epitaxy (MBE). See References 9-15.
  • MBE molecular beam epitaxy
  • the film growth reported by these early efforts did not utilize a low temperature buffer layer and did not possess smooth planar surfaces, and therefore, these layers were poorly suited for heterostructure growth and analysis. Consequently, there is a need for improved methods of growing films that exhibit improved surface and structural quality as compared to previously reported growth of GaN on r-plane sapphire via MOCVD.
  • the present invention describes a method for growing device-quality non-polar aplane GaN thin films via MOCVD on r-plane sapphire substrates.
  • the present invention provides a pathway to nitride-based devices free from polarization-induced effects, since the growth direction of non-polar a-plane GaN thin films is perpendicular to the polar c-axis.
  • Polarization-induced electric fields will have minimal effects, if any, on (Al,B,In,Ga)N device layers grown on non-polar a-plane GaN thin films.
  • FIG. 1 is a flowchart that illustrates the steps of the MOCVD process for the growth of non-polar (11 ⁇ overscore (2) ⁇ 0) a-plane GaN thin films on (1 ⁇ overscore (1) ⁇ 20) r-plane sapphire, according to the preferred embodiment of the present invention
  • FIG. 2( a ) shows a 2 ⁇ - ⁇ diffraction scan that identifies the growth direction of the GaN film as (1 ⁇ overscore (1) ⁇ 20) a-plane GaN;
  • FIG. 2( b ) is a compilation of off-axis ⁇ scans used to determine the in-plane epitaxial relationship between GaN and r-sapphire, wherein the angle of inclination ⁇ used to access the off-axis reflections is noted for each scan;
  • FIG. 2( c ) is a schematic illustration of the epitaxial relationship between the GaN and r-plane sapphire
  • FIGS. 3 ( a ) and 3 ( b ) are cross-sectional and plan-view transmission electron microscopy (TEM) images, respectively, of the defect structure of the a-plane GaN films on r-plane sapphire; and
  • FIGS. 4 ( a ) and 4 ( b ) are atomic force microscopy (AFM) amplitude and height images, respectively, of the surface of the as-grown a-plane GaN films.
  • AFM atomic force microscopy
  • the present invention describes a method for growing device quality non-polar (11 ⁇ overscore (2) ⁇ 0) a-plane GaN thin films via MOCVD on (1 ⁇ overscore (1) ⁇ 02) r-plane sapphire substrates.
  • the method employs a low-temperature buffer layer grown at atmospheric pressure to initiate the GaN growth on r-plane sapphire. Thereafter, a high temperature growth step is performed at low pressures, e.g., ⁇ 0.1 atmospheres (atm) in order to produce a planar film.
  • Planar growth surfaces have been achieved using the present invention. Specifically, the in-plane orientation of the GaN with respect to the r-plane sapphire substrate has been confirmed to be [0001] GaN ⁇ [ ⁇ overscore (1) ⁇ 101] sapphire and ⁇ [ ⁇ overscore (1) ⁇ 100] GaN ⁇ [11 ⁇ overscore (2) ⁇ 0] sapphire .
  • the resulting films possess surfaces that are suitable for subsequent growth of (Al,B,In,Ga)N device layers. Specifically, polarization-induced electric fields will have minimal effects, if any, on (Al,B,In,Ga)N device layers grown on non-polar a-plane GaN base layers.
  • FIG. 1 is a flowchart that illustrates the steps of the MOCVD process for the growth of non-polar (11 ⁇ overscore (2) ⁇ 0) a-plane GaN thin films on a (1 ⁇ overscore (1) ⁇ 20) r-plane sapphire substrate, according to the preferred embodiment of the present invention.
  • the growth process was modeled after the two-step process that has become the standard for the growth of c-GaN on c-sapphire. See Reference 16.
  • Block 100 represents loading of a sapphire substrate into a vertical, close-spaced, rotating disk, MOCVD reactor.
  • epi-ready sapphire substrates with surfaces crystallographically oriented within +/ ⁇ 2° of the sapphire r-plane (1 ⁇ overscore (1) ⁇ 20) may be obtained from commercial vendors. No ex-situ preparations need be performed prior to loading the sapphire substrate into the MOCVD reactor, although ex-situ cleaning of the sapphire substrate could be used as a precautionary measure.
  • Block 102 represents annealing the sapphire substrate in-situ at a high temperature (>1000° C.), which improves the quality of the substrate surface on the atomic scale. After annealing, the substrate temperature is reduced for the subsequent low temperature nucleation layer deposition.
  • Block 104 represents depositing a thin, low temperature, low pressure, nitride-based nucleation layer as a buffer layer on the sapphire substrate.
  • the nucleation layer is comprised of, but is not limited to, 1-100 nanometers (nm) of GaN and is deposited at low temperature, low pressure depositing conditions of approximately 400-900° C. and 1 atm.
  • Such layers are commonly used in the heteroepitaxial growth of c-plane (0001) nitride semiconductors. Specifically, this depositing step initiates GaN growth on the r-plane sapphire substrate.
  • Block 106 represents growing the non-polar (11 ⁇ overscore (2) ⁇ 0) a-plane GaN thin films on the substrate.
  • the high temperature growth conditions comprise, but are not limited to, approximately 1100° C. growth temperature, approximately 0.2 atm or less growth pressure, 30 ⁇ mol per minute Ga flow, and 40,000 ⁇ mol per minute N flow, thereby providing a V/III ratio of approximately 1300).
  • the precursors used as the group III and group V sources are trimethylgallium and ammonia, respectively, although alternative precursors could be used as well.
  • growth conditions may be varied to produce different growth rates, e.g., between 5 and 9 ⁇ per second, without departing from the scope of the present invention.
  • Non-polar GaN approximately 1.5 ⁇ m thick have been grown and characterized.
  • Block 108 represents cooling the non-polar (11 ⁇ overscore (2) ⁇ 0) a-plane GaN thin films under a nitrogen overpressure.
  • Block 110 represents the end result of the processing steps, which is a nonpolar (11 ⁇ overscore (2) ⁇ 0) a-plane GaN film on an r-plane sapphire substrate.
  • Potential device layers to be manufactured using these process steps to form a non-polar (11 ⁇ overscore (2) ⁇ 0) a-plane GaN base layer for subsequent device growth include laser diodes (LDs), light emitting diodes (LEDs), resonant cavity LEDs (RC-LEDs), vertical cavity surface emitting lasers (VCSELs), high electron mobility transistors (HEMTs), heterojunction bipolar transistors (HBTs), heterojunction field effect transistors (HFETs), and UV and near-UV photodetectors.
  • LDs laser diodes
  • LEDs light emitting diodes
  • RC-LEDs resonant cavity LEDs
  • VCSELs vertical cavity surface emitting lasers
  • HEMTs high electron mobility transistors
  • HBTs heterojunction bipolar transistors
  • HFETs hetero
  • FIG. 2( a ) shows a 2 ⁇ - ⁇ diffraction scan that identifies the growth direction of the GaN film as (11 ⁇ overscore (2) ⁇ 0) a-plane GaN.
  • the scan detected sapphire (1 ⁇ overscore (1) ⁇ 02), (2 ⁇ overscore (2) ⁇ 04), and GaN (11 ⁇ overscore (2) ⁇ 0) reflections.
  • FIG. 2( b ) is a compilation of off-axis ⁇ scans used to determine the in-plane epitaxial relationship between GaN and r-sapphire, wherein the angle of inclination ⁇ used to access the off-axis reflections is noted for each scan. Having confirmed the a-plane growth surface, off-axis diffraction peaks were used to determine the in-epitaxial relationship between the GaN and the r-sapphire.
  • FIG. 2( c ) is a schematic illustration of the epitaxial relationship between the GaN and r-plane sapphire.
  • the a-GaN polarity was determined using CBED. The polarity's sign is defined by the direction of the polar Ga—N bonds aligned along the GaN c-axis; the positive c-axis [0001] points from a gallium atom to a nitrogen atom. Consequently, a gallium-face c-GaN film has a [0001] growth direction, while a nitrogen-face c-GaN crystal has a [000 ⁇ overscore (1) ⁇ ] growth direction.
  • GaN is aligned with the sapphire c-axis projection [ ⁇ overscore (1) ⁇ 101] sapphire , and therefore, the epitaxial relationships defined above are accurate in terms of polarity. Consequently, the positive GaN c-axis points in same direction as the sapphire c-axis projection on the growth surface (as determined via CBED). This relationship concurs with the epitaxial relationships previously reported by groups using a variety of growth techniques. See References 9, 12 and 14. Therefore, the epitaxial relationship is specifically defined for the growth of GaN on an r-plane sapphire substrate.
  • FIGS. 3 ( a ) and 3 ( b ) are cross-sectional and plan-view TEM images, respectively, of the defect structure of the a-plane GaN films on an r-plane sapphire substrate. These images reveal the presence of line and planar defects, respectively.
  • the cross-sectional TEM image in FIG. 3( a ) reveals a large density of threading dislocations (TD's) originating at the sapphire/GaN interface with line directions parallel to the growth direction [11 ⁇ overscore (2) ⁇ 0].
  • the TD density determined by plan view TEM, was 2.6 ⁇ 10 10 cm ⁇ 2 .
  • the plan view TEM image in FIG. 3( b ) reveals the planar defects observed in the a-GaN films.
  • Stacking faults aligned perpendicular to the c-axis with a density of 3 . 8 ⁇ 10 5 cm ⁇ 1 were observed in the plan-view TEM images.
  • Stacking faults with similar characteristics were observed in a-plane AlN films grown on r-plane sapphire substrates. See Reference 17.
  • the stacking faults have a common faulting plane parallel to the close-packed (0001) and a density of ⁇ 3.8 ⁇ 10 5 cm ⁇ 1 .
  • on-axis peak widths are broadened by screw and mixed dislocations, while off-axis widths are broadened by edge-component TD's (assuming the TD line is parallel to the film normal). See Reference 18.
  • edge-component TD's assuming the TD line is parallel to the film normal.
  • FIGS. 4 ( a ) and 4 ( b ) are AFM amplitude and height images, respectively, of the surface of the as-grown a-plane GaN film.
  • the surface pits in the AFM amplitude image of FIG. 4( a ) are uniformly aligned parallel to the GaN c-axis, while the terraces visible in the AFM height image of FIG. 4( b ) are aligned perpendicular to the c-axis.
  • the a-GaN growth surface is pitted on a sub-micron scale, as can be clearly observed in the AFM amplitude image shown in FIG. 4( a ). It has been proposed that the surface pits are decorating dislocation terminations with the surface; the dislocation density determined by plan view TEM correlates with the surface pit density within an order of magnitude.
  • the nucleation layer deposition is crucial to achieving epitaxial GaN films with smooth growth surfaces and minimal crystalline defects.
  • use of AlN or AlGaN nucleation layers in place of GaN could prove useful in obtaining high quality a-plane GaN films.
  • non-polar a-plan GaN thin films are described herein, the same techniques are applicable to non-polar m-plane GaN thin films. Moreover, non-polar InN, AlN, and AlInGaN thin films could be created instead of GaN thin films.
  • substrates other than sapphire substrate could be employed for non-polar GaN growth.
  • These substrates include silicon carbide, gallium nitride, silicon, zinc oxide, boron nitride, lithium aluminate, lithium niobate, germanium, aluminum nitride, and lithium gallate.
  • the present invention describes the growth of non-polar (11 ⁇ overscore (2) ⁇ 0) a-plane GaN thin films on r-plane (1 ⁇ overscore (1) ⁇ 02) sapphire substrates by employing a low temperature nucleation layer as a buffer layer prior to a high temperature growth of the epitaxial (11 ⁇ overscore (2) ⁇ 0) a-plane GaN films.
  • the epitaxial relationship is [0001] GaN ⁇ [ ⁇ overscore (1) ⁇ 101] sapphire and [ ⁇ overscore (1) ⁇ 100] GaN ⁇ [11 ⁇ overscore (2) ⁇ 0] sapphire with the positive GaN c-axis pointing in the same direction as the sapphire c-axis projection on the growth surface.

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US10/413,691 US20030198837A1 (en) 2002-04-15 2003-04-15 Non-polar a-plane gallium nitride thin films grown by metalorganic chemical vapor deposition
CN2003801109995A CN1894771B (zh) 2003-04-15 2003-12-11 非极性(Al,B,In,Ga)N量子阱
JP2005512863A JP5096677B2 (ja) 2003-04-15 2003-12-11 非極性（Ａｌ、Ｂ、Ｉｎ、Ｇａ）Ｎ量子井戸
US10/582,390 US20070128844A1 (en) 2003-04-15 2003-12-11 Non-polar (a1,b,in,ga)n quantum wells
EP03790447A EP1697965A4 (fr) 2003-04-15 2003-12-11 Puits quantiques (a1, b, in, ga)n non polaires
AU2003293497A AU2003293497A1 (en) 2003-04-15 2003-12-11 Non-polar (a1,b,in,ga)n quantum wells
PCT/US2003/039355 WO2005064643A1 (fr) 2003-04-15 2003-12-11 Puits quantiques (al, b, in, ga)n non polaires
US11/140,893 US7208393B2 (en) 2002-04-15 2005-05-31 Growth of planar reduced dislocation density m-plane gallium nitride by hydride vapor phase epitaxy
US13/151,491 US9039834B2 (en) 2002-04-15 2011-06-02 Non-polar gallium nitride thin films grown by metalorganic chemical vapor deposition
US14/921,734 US9893236B2 (en) 2002-04-15 2015-10-23 Non-polar (Al,B,In,Ga)N quantum wells

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US11/140,893 Continuation-In-Part US7208393B2 (en) 2002-04-15 2005-05-31 Growth of planar reduced dislocation density m-plane gallium nitride by hydride vapor phase epitaxy
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US10/413,690 Expired - Lifetime US7091514B2 (en) 2002-04-15 2003-04-15 Non-polar (Al,B,In,Ga)N quantum well and heterostructure materials and devices
US11/472,033 Active 2024-08-19 US7982208B2 (en) 2002-04-15 2006-06-21 Non-polar (Al,B,In,Ga)N quantum well and heterostructure materials and devices
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US13/151,491 Expired - Lifetime US9039834B2 (en) 2002-04-15 2011-06-02 Non-polar gallium nitride thin films grown by metalorganic chemical vapor deposition
US13/457,032 Abandoned US20120205623A1 (en) 2002-04-15 2012-04-26 NON-POLAR (Al,B,In,Ga)N QUANTUM WELL AND HETEROSTRUCTURE MATERIALS AND DEVICES

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US13/099,834 Expired - Lifetime US8188458B2 (en) 2002-04-15 2011-05-03 Non-polar (Al,B,In,Ga)N quantum well and heterostructure materials and devices
US13/151,491 Expired - Lifetime US9039834B2 (en) 2002-04-15 2011-06-02 Non-polar gallium nitride thin films grown by metalorganic chemical vapor deposition
US13/457,032 Abandoned US20120205623A1 (en) 2002-04-15 2012-04-26 NON-POLAR (Al,B,In,Ga)N QUANTUM WELL AND HETEROSTRUCTURE MATERIALS AND DEVICES

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